Thermo-derivative analysis of Al–Si–Cu alloy used for surfacetreatment

Krzysztof Labisz1• Jarosław Konieczny1

• Sebastian Jurczyk3• Tomasz Tanski2 •

Mariusz Krupinski2

Received: 19 June 2016 / Accepted: 15 February 2017

� The Author(s) 2017. This article is published with open access at Springerlink.com

Abstract The only effective way to design, produce,

analyse and optimise new and existing industrial thermal

processes and also laser-based processes is to develop a

quantitative knowledge and understanding of the depen-

dence between temperature and time, which allow the

desired forming of properties of the final products. The

purpose of this paper was the performance of thermo-

derivative analysis using the UMSA platform of alu-

minium alloy cooled at chosen rate, for obtaining char-

acteristics used later for laser treatment and its influence

on the microstructure and properties of the surface layer

of heat-treated Al–Si–Cu cast aluminium alloys, using the

high-power diode laser. The performed laser treatment

involves remelting and feeding of ceramic powder into the

aluminium surface. The carried out investigations allow to

conclude that as a result of alloying of the heat-treated

cast aluminium alloys with oxide ceramic powder, a

surface layer was obtained with higher hardness compared

to non-laser-treated material. The surface layer can be

enriched with the powder particle, and in some cases a

high-quality top layer is possible to obtain. Also a

microstructure refinement of the surface layer was

achieved due to the high laser power use and conse-

quently high cooling rate during the crystallisation pro-

cess. Concerning original practical implications of this

work, there was important to investigate the appliance

possibility of thermal analysis for further surface treat-

ment for enhancement of the aluminium surface proper-

ties, especially the wear resistance and hardness. The

scientific reason was also to describe microstructure

changes and processes occurred in the laser remelted

surface aluminium layer after laser treatment.

Keywords Manufacturing and processing � Surfacetreatment � Thermo-derivative analysis � Aluminium

alloys � UMSA

Introduction

Aluminium alloys are especially preferred in designs

thanks to their good mechanical properties and possibility

to make very complicated castings with high service

properties. A new approach on enhancing the existing

properties can be the appliance of thermo-derivative

methods for further surface treatment. Nowadays alu-

minium alloys play an increasingly role in the world con-

structional material production, because of the availability

and properties which are possible to obtain. Mechanical

properties of the Al–Si alloys are dependent on the size,

shape and distribution of the Si eutectic present in the

microstructure. Improvement of the mechanical properties

of these alloys is realised by general modification. Change

of the fibrous Si morphology makes it possible to achieve

better mechanical properties of the Al–Si alloys [1, 2].

A newly developed investigation technology is the

application of derivative thermo-analysis using the

& Krzysztof Labisz

krzysztof.labisz@polsl.pl

1 Faculty of Transport, Silesian University of Technology,

Krasinskiego 8, 40-019 Katowice, Poland

2 Division of Materials Processing Technology, Management

and Computer Techniques in Materials Science, Institute of

Engineering Materials and Biomaterials, Silesian University

of Technology, Konarskiego Str 18A, 44-100 Gliwice,

Poland

3 Paint and Plastics Department, Institute for Engineering of

Polymer Materials and Dyes, Chorzowska Str 50A,

44-100 Gliwice, Poland

123

J Therm Anal Calorim

DOI 10.1007/s10973-017-6204-9

Universal Metallurgical Simulator and Analysator. The

UMSA device used for investigations is designed to

overcome the existing problem of laboratory and industrial

equipment on the present market. This platform combines

computer controlled melting and heat treatment devices

with a quench equipment, as well as the device for thermal

analysis and testing equipment for in situ investigations of

test sample crystallization characteristics [4–6].

This method can deliver important insight into the alloy

thermal processes, which could be helpful determining the

usability of the alloys for further treatment, for example

surface treatment using laser. One of themodernmethods for

surface layer engineering is currently laser surface treatment.

In this method, to the matrix there are introduced small

amount of alloying additions into the surface layer in form of

ceramic particle powders with different properties changing

the surface layer application possibilities. The laser treat-

ment as a part of the new generation techniques applied in

metal surface technology is discussed in this paper. One of

the intrinsic/distinctive high-power diode laser (HPDL)

properties is the rectangular beam shape, which can be

profitably used in welding of large polymer parts. Polymer

welding with a single moving HPDL beam was one of the

earliest applications. Welding operations can be performed

simultaneously when a single scanable beam is replaced by

several larger rectangular beams. HPDL is the most pro-

ductive artificial light sources which a significant part of the

electrical energy is converted to heat in the diode laser.

In real conditions, the crystallization of the Al alloys

shows departures of the crystallization process resulting

from the Al–Si equilibrium diagram, which is a binary

system with an eutectic and limited solubility of the com-

ponents in a solid state. The reason of this difference is the

considerably higher alloy crystallization rate, compared to

this occurred in equilibrium conditions, but also the change

in the initial alloy microstructure in the liquid state, caused

by impurities, or specially added modifiers for the reason of

microstructure modification and morphology changes of the

(aAl ? bSi) eutectic or shifting of the characteristic equi-

librium diagram temperature points, because of the pressure

increase during the alloy crystallisation process. In this area,

also the HPDL laser treatment with ceramic particle feeding

is of big importance for changing the microstructure of

aluminium [7–14]. The field of use of such HPDL-treated

surface is repair of working elements produced from alu-

minium, where enhanced hardness and wear resistance is of

great importance, for example valve seats or motor housing

and pulley system parts.

Exact knowledge of the impact of the cooling rate

applied for die castings on the microstructure and phase

transition temperature during non-equilibrium crystalliza-

tion allows optimal control of the production process. The

separation of the derivative curve definitions to basic

functions allows accurate calculation of latent crystalliza-

tion heat of various phases crystallising during solidifica-

tion. Assuming that the latent crystallization heat is

proportional to the share of the various phases in the alloy,

the thermo-derivative analysis also allows the calculation

of the amount of crystallised phases. Calculation of the

above-mentioned properties is based on the characteristic

points determined in a derivative curve. These points are

usually reflecting the thermal effects occurring in the melt

during crystallization and are dependent on the alloy

composition, cooling rate, heat generation rate and crys-

tallization temperature of the molten metal, and so the

parameters affecting the final microstructure of the result-

ing alloy. These parameters characterise also the crystal-

lization kinetics of the alloys.

The general equation, describing (Table 1) the crys-

tallisation function as a derivative of the crystallisation, is

given as (1) [3, 4]:

dT

dt¼ A

m� cp� a tð Þ � T � T0ð Þ þ KK

m� cp

� mdz

dtþ z

dm

dt

� �ð1Þ

The basic laser treatment parameters are the practical

aim of this work, as well as improvement of hardness.

Special attention was payed to studying of the surface layer

morphology of the investigated material especially the

surface layer microstructure [15–30] if the used ceramic

particle powder was properly introduced into the matrix,

how the phases were changed in terms of distribution and

size as well as if a zone-like structure was obtained after

appliance of the laser surface treatment.

Experimental

The material used for investigation was the AlSi7Cu and

AlSi9Cu4 aluminium alloys. The chemical compositions of

the investigated aluminium alloys are presented in Table 2,

as obtained by the manufacturer. For feeding of both of the

material types, the zirconium oxide ZrO2 and titanium

Table 1 Description of the equation factors

Symbol Descriptions

cp Heat capacity

m Mass of the crystallised metal

T Temperature at time dt

TO Environment temperature

A Sampler surface

KK Crystallisation constant

z Nucleus number

K. Labisz et al.

123

carbide TiC mixed powders were used in a ration 50–50%

by a fluidisation feeder mounted on the lasers head.

The heat treatment for both alloys was carried out in the

electric resistance furnace U117, with a heating rate of

80 �C s-1 for the ageing process and 300 �C s-1 for the

solution heat treatment process with two holds at 300 and

450 �C performed for 15 min. Parameters of the solution

heat treatment process and ageing process are presented in

Table 3.

Thermo-analysis of the investigated alloy was carried

out using UMSA device. The heating and cooling system,

with experimental conditions, is presented in Fig. 1. The

samples were cooled using compressed gas supplied

through the nozzles present in the heating inductor. The gas

flowing rate for sample cooling was regulated and con-

trolled using a rotameter. The compressed gas flow rate

was regulated for achieving the cooling rate of 0.1 �C s-1

for furnace cooled sample.

For measurement, K-type (chromo–alumel) thermocou-

ples were used. Tests were performed several times for

each cooling rate for statistical estimation of the investi-

gation results.

High-power diode laser HPDL Rofin DL 020 was used

for remelting. The used laser is a device with high power,

used in materials science, including for welding. The laser

equipment contained: rotary table which moving in the XY

plane, the nozzle of the powder feeder for the enrichment

or welding, shielding gas nozzle, laser head, power system,

cooling system and the computer system controlling the

operation and location of the laser. The powder feed rate

was chosen as 1 g min-1 and the laser scan rate

0.5 m min-1. Working parameters of the HPDL Rofin DL

020 are shown in Table 4.

For determining the influence of cooling rate on the

further surface layer properties, the following investiga-

tions were carried out:

• Thermo-derivative analysis using the UMSA thermo

simulator (Fig. 1).

• The micrographs of the microstructure investigation

were performed using the light microscope Leica

MEF4A supplied by Zeiss in a magnification range of

50–500 times. The micrographs of the microstructures

were made by means of the KS 300 program using the

digital camera equipped with a special image software.

Also the intern image calculation software was used for

calculation of the phases present in the microstructure.

• The obtained results from the microstructure investi-

gation were performed on the scanning electron

microscope ZEISS Supra 35 with a magnification up

to 2500 times, as well as on a transmission electron

Table 2 Chemical composition of the investigated aluminium alloys

Elements Chemical composition

Alloys AlSi7Cu AlSi9Cu4

Si 7.17 7.45

Fe 0.14 0.17

Cu 0.99 3.60

Mn 0.11 0.25

Mg 0.27 0.28

Zn 0.05 0.06

Ti 0.08 0.13

Al Balance Balance

Chemical composition of the investigated alloys, in mass %

Table 3 Heat treatment parameters

Ageing process Solution heat treatment

Temperature 175 �C for 12 h Temperature 505 �C for 10 h

Heating rate 80 �C s-1 Heating rate 300 �C s-1

Isothermal holds 450 �C by 15 min Isothermal holds 450 �C by 15 min

Isothermal holds 300 �C by 15 min Isothermal holds 300 �C by 15 min

Cooling medium Air Cooling medium Water

Heat treatment parameters used for the investigated AlSi9Cu4 and AlSi7Cu alloys

1

2

3

4

5

Fig. 1 UMSA device location scheme of the heating and cooling

system, as well as size of the samples for thermo-analysis:

(1) thermocouple, (2) heating inductor—cooling nozzles, (3) steel

foil, (4) sample, (5) sampler isolation

Thermo-derivative analysis of Al–Si–Cu alloy used for surface treatment

123

microscope with the high-angle annular dark-field

(HAADF) mode. For microstructure evaluation, the

back-scattered electrons (BSE) as well as the secondary

electron (SE) detection method was used, with the

accelerating voltage of 20 kV.

• The hardness was measured with Rockwell hardness

tester with a load chosen for the HRF scale, with a load

of 600 N, predestined for light alloy hardness testing.

Results and discussion

The obtained results from the microstructure investigation

performed on scanning electron microscope ZEISS Supra 35

with a magnification up to 500 times reveal the cross-sectional

Table 4 HPDL laser working parameters

Parameter Value

Laser wavelength/nm 940 ± 5

Peak power/W 100 ? 2300

Focus length of the laser beam/mm 82/32

Power density range of the laser beam in

the focus plane/kW (cm2)-10.8/36.5

Dimensions of the laser beam focus/mm 1.8 9 6.8/1.8 9 3.8

Laser scan rate/m min-1 2

Powder feed rate/g min-1 5

1.5 mm

Fig. 2 Cross section of the investigated AlSi9Cu4 surface layer after

laser treatment ZrO2 ? TiC, laser power 1.5 kW

1 mm

(a)

(b)

Fig. 3 Microstructure of the investigated AlSi7Cu alloy, ZrO2 ?

TiC, 1.5 kW (a), transition zone between the heat influence zone and

the substrate material (b)

1 mm

(a)

(b)

Fig. 4 Microstructure of the investigated AlSi9Cu4 alloy, ZrO2 ?

TiC, 1.5 kW (a), transition zone between the remelting zone and heat

influence zone (b)

βSi

Al2CuAl-Si-Cu-Mg

eutectic

αAl

Fig. 5 Microstructure of the AlSi9Cu4, as-cast state, cooled sample

with 0.1 �C s-1

K. Labisz et al.

123

structure (Fig. 2) of the surface layer, revealing the remelting

zone (RZ) as well as the presence of the used ZrO2 powder in

form of a film (Figs. 3, 4)—discontinuous for the AlSi7Cu

alloy. In case of this powder, the particles are sintered building

a layer on the top of the laser-treated aluminium surface and

are not emerged in the matrix. For microstructure evaluation,

the back-scattered electrons (BSE) detection method was used,

with the accelerating voltage of 20 kV.

The morphology of the resulting quasi-composite layer

tends to be not homogeny and entered the correct disper-

sion of particles throughout the depth of penetration with

the exception of a very thin layer of diffusion saturation;

therefore, it is very important to know which structural

features and microstructure elements can be present in

different thermal conditions.

The occurred discontinuity of the layer can be seen as a

product of the heat transfer process and may be neutralised

by properly adjusted powder quality and powder feed rate.

It is also possible on the basis of these cross-sectional

micrographs to evaluate the thickness of the surface layer

depth, which is ca. 0.7 lm (Fig. 9) in case of the AlSi9Cu4alloy. For the AlSi7Cu alloy, the obtained microstructure

investigation results allow to confirm only a minor amount

of the ZrO2 powder on the surface of the treated alloy. It

was also found that the examined layers consist of three

βSi

Al2Cu

αAl

Al5FeSi

Fig. 6 Microstructure of the AlSi7Cu, as-cast state, cooled sample

with 0.1 �C s-1

100 nm

Fig. 7 Microstructure of the investigated Al alloy, revealing the

Mg2Si phase, HAADF-TEM

Fig. 8 Electron diffraction pattern forms the phase in Fig. 7, with

solution for the Mg2Si phase, [001] zone axis, TEM

0

0.2

0.4

0.6

0.8

AISi7Cu

AISi9Cu4

Substrate material

0.25

0.7

Sur

face

laye

r de

pth/

mm

Fig. 9 Surface layer depth measurement results of the alloyed cast

aluminium alloys with ZrO2/TiC ceramic powder

AISi7Cu

AISi9Cu4

Substrate material

Sur

face

laye

r ha

rdne

ss, H

RF

74

72

70

686664

6260

65

69

73

67

as-cast Laser treated

Fig. 10 Surface layer hardness measurement results of the alloyed

cast aluminium alloys with ZrO2/TiC ceramic powder

Thermo-derivative analysis of Al–Si–Cu alloy used for surface treatment

123

subzones—the remelted zone, the heat influence zone and

the substrate material. Further investigations will be needed

to reveal the morphology and nature of these zones,

occurring after alloying with different process parameters

and different ceramic powders.

It is known that the coarseness of the as-cast

microstructure (Figs. 5, 6) clearly affects the solution

treatment time needed to dissolve particles and obtain a

homogenous distribution of alloying elements in the

matrix. A short solution treatment time of 10 min is enough

to achieve a high and homogenous copper concentration

for a material with a fine microstructure.

There is also a different phase composition in the ther-

mally treated alloys; in case of the as-cast AlSi7Cu alloy,

there are common Al5FeSi and Al2Cu phases present,

whereas in the AlSi9Cu4 alloy occurs also in a higher

amount of the AlSiCuMg multiphase eutectic, consisting of

the Al2Cu and Al5FeSi phases, as well as of a magnesium

and silicon-containing phase Mg2Si (Figs. 7 and 8).

The uneven areas and hollows in the surface layer of the

Al–Si-Cu alloys with laser-alloyed zirconium oxide parti-

cles are produced as a result of intensive heating of the

surface. Depending on the type of substrate, laser power,

feed rate and the powder applied, the surface on which high

Exo direction of heat transport with positive coolingrate values

100 200 300 400 500 600 700 800 900 1000 1100 1200

Time/s

800

750

700

650

600

550

500

450

400

350

300

Tem

pera

ture

/°C

Cooling curveDerivative curve

Base line

1.0

0.5

0.0

–0.5

–1.0

–1.5

–2.0

Coo

ling

rate

/°C

s–1

I

II

III

IV

VIVII

V

TDN

TE(AI+Si)T(AI+Si+Cu)

T(AI+Si+Cu+Mg)

Tsol

Fig. 11 Thermo-derivative

analysis of the AlSi7Cu alloy

Exo direction of heat transport with positive coolingrate values

100 200 300 400 500 600 700 800 900

Time/s

800

700

600

500

400

300

200

Tem

pera

ture

/°C

Cooling curve

Derivative curveBase line

0.5

0.0

–0.5

–1.0

–1.5

–2.0

I

II

III

IV

VIVII

V

TDN TE(AI+Si)T(AI+Si+Cu)

T(AI+Si+Cu+Mg)

Tsol

Coo

ling

rate

/°C

s–1

Fig. 12 Thermo-derivative

analysis of the AlSi9Cu4 alloy

K. Labisz et al.

123

gradient of surface tension is produced is unevenly heated,

which has a direct influence on the formation of the melted

material in the remelting lake.

Some of the alloy and ceramic parts embedded in the

remelting zone are evaporated under high temperature

occurring during laser treatment; therefore, the character-

istic hollows appear on the remelting surface. It was also

found that, disregarding the ceramic powder used, in the

laser bundle power range from 1.2 to 2.0 kW the porosity

of the obtained composite layers increases, in comparison

with that of the raw cast surfaces of aluminium alloys.

The silicon particles, present as coarse, acicular needles

under normal cooling conditions, act as crack initiators but

enhance the hardness. A higher influence on the hardness

increase can be observed based on the comparison between

as-cast and HPDL-treated samples, where for the laser-

treated sample the hardness increase an even more clear,

equal 73 HRF for the AlSi9Cu4 alloy, influenced also by

higher grain refinement (Fig. 10).

There is obviously a clear relationship between the laser

power applied and the achieved quality of the laser-treated

surface, and the particular investigation concerning laser

power influence were carried out in former works [3, 4]. It

was found that the optimal laser power is ca. 1.5 kW.

Higher addition of silicon and copper in alloy caused

change in the derivative curve (Figs. 11, 12). Higher

amount of silicon and copper affects the position of the

characteristic points of the beginning and end of solidifi-

cation of the eutectic phases. Figure 11 shows an example

of the cooling curves and derivative curves of the AlSi7Cu

alloys. In this case, there is no evidence of occurring of any

other phases than commonly known, whereas for the

AlSi9Cu4 alloy there is a clear area in the curve marked

with points VI (nucleation temperature of the (Al–Si–Cu–

Mg) multiphase eutectic) (Table 5) where the multiphase

eutectic occurs. Change of the derivative curve effects also

the area under the curve and the ratio of the various phases

and eutectic according to the chemical composition and

cooling rate. For example, for the AlSi9Cu4 alloy the

occurrence of the Al–Si–Cu–Mg eutectic was confirmed, as

well as the amount of the Si phase was measured as 8.43%

compared to 5.64% for the AlSi7Cu alloy.

Very important issue is also the crystallisation end

temperature for the investigated alloys. This TSol temper-

ature is ca 465 �C for the AlSi7Cu alloy and ca 455 �C for

the AlSi9Cu4 alloy. The maximal heating temperature is

much more higher than the TL (liquidus) temperature for

both types of the investigated alloys because of the

necessity to have information about the solidification pro-

cess and phase transformations occurred on the beginning

of the alloy solidification—ca. 650 �C for the beginning of

the crystal growth (a phase dendrites). Such high temper-

ature was also chosen, because of the following laser

treatment, where the metal surface if entire remelted, and

some crystallization process could have placed in higher

temperature, compared to the classical phase transforma-

tion diagram.

On the basis of these data, an undercooling for this alloy

can be stated, where the alloy solidifies in lower temper-

ature, than given in the equilibrium diagram. Such under-

cooling occurs also after the laser alloying of the surface

layer, where the temperature reaches even 3000 �C. So a

higher amount of alloying additives can lead to a presence

of the phase composition of the alloy and a higher possi-

bility for heat transfer, by this way alloys with higher

alloying element content, and also impurities are more

likely to be used for laser surface treatment.

Conclusions

Control of the hypo-eutectic alloy microstructures is

imperative in the design of both superior hardness tribo-

logical properties at the bore surface and for exceptional

mechanical strength. However, the solidification kinetics

and the sequence of the phase transformations in relation to

the as-cast and heat-treated microstructure needs still to be

further understood, quantified and implemented for further

improvement of the casting technology and cast compo-

nent service characteristics. The performed investigations

of the microstructure evaluation of the Al–Si–Cu alloys,

carried out using light and scanning electron microscope,

allow to confirm the zone-like nature of the surface layer

obtained using HPDL laser for alloying of the AlSi7Cu as

well as the AlSi9Cu4 cast aluminium alloys. There were

revealed also a zone-like nature on the top of the substrate

material, like: the remelting zone and the heat influence

zone.

Table 5 Description of the characteristic points on the cooling curve

from Figs. 9 and 10

Point on

the graph

Description

I TDN nucleation temperature

II T temperature of the beginning of the crystal growth

(a phase dendrites)

III Dendrites (a phase) growth temperature

IV Temperature of a phase dendrite growth and

(aAl ? bSi) precipitation growth

V Nucleation temperature of the (Al–Si–Cu) eutectics

VI Nucleation temperature of the (Al–Si–Cu–Mg)

multiphase eutectic

VII TSol temperature of the crystallization end

Thermo-derivative analysis of Al–Si–Cu alloy used for surface treatment

123

The investigated hypo-eutectic Al–Si alloys are near

eutectic Al–Si alloys with the addition of copper and small

addition of iron and magnesium, reveal the occurrence of

formation of aluminium reach (a-Al) dendrites followed by

development of three phases which are of importance for

achieving the required properties after properly performed

heat treatment, these are: the Si phase, the Al2Cu phase as

well as the Al5FeSi phase. However, the additional alloying

elements Fe, Mg, Cu lead to more complex solidification

reaction, partially unidentified.

Crystallization of the investigated Al–Si alloy starts with

the crystallization of a-Al, followed by aAl ? bSi eutec-tic; silicomanganese FeSiMn phase. There are some indi-

ces, mainly on the thermal analysis curve, that some less

often occurred phases are present in this alloy for example

the Mg2Si phase, which was confirmed using the electron

diffraction method on the transmission electron

microscope.

Cooling rate has an important influence on the hardness,

which has a value of 73 HRF for the samples cooled with

0.1 �C s-1.

Particularly, it was found that:

1. The optimal laser power is in the range of

\1.0–2.0[ kW.

2. The ZrO2\TiC powder particles do not feed into the

aluminium alloy matrix during laser alloying, instead

there is formed a sintered ZrO2 layer onto the

investigated aluminium cast alloy, the presence of

the titanium carbide phase could not be detected in the

microstructure or using EDS analysis. It is probably

evaporated during the laser feeding process.

3. The AlSi9Cu4 alloy has a more homogeny surface

layer depth after alloying compared to the AlSi7Cu

aluminium alloy.

The laser power determination leads to the conclusion,

that the optimal power range is ca. 1.5 kW, a lower value

of ca 1.0 kW does not lead to achievement of an com-

pletely homogeny remelting tray on the sample surface,

whereas a to high power of 2.0 kW makes an uneven,

bumpy or hilly shape of the remelted area.

Acknowledgements This publication was financed by the Ministry of

Science and Higher Education of Poland as the statutory Financial

Grant of the Faculty ofMechanical EngineeringSUT.This researchwas

also partially financed partially within the framework of the Scientific

Research Project No. 2011/01/B/ST8/06663 headed by Dr. KL.

Open Access This article is distributed under the terms of the

Creative Commons Attribution 4.0 International License (http://crea

tivecommons.org/licenses/by/4.0/), which permits unrestricted use,

distribution, and reproduction in any medium, provided you give

appropriate credit to the original author(s) and the source, provide a

link to the Creative Commons license, and indicate if changes were

made.

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